Reaktion #63647

ord-db1c7b5655734fdd82605a2897516b93

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe reaction mixture was refluxed overnight
  2. 2
    Sonstigedimethylformamide was evaporated under reduced pressure
  3. 3
    Extraktionthe residue was extracted with methylene chloride (400 ml.)
  4. 4
    SonstigeThe methylene chloride extracts were collected
  5. 5
    Waschenwashed with water
  6. 6
    Sonstigeevaporated
  7. 7
    Sonstigethe remaining residue was purified by HPLC
  8. 8
    Sonstigeto give 1.3 g

Vorschrift

To a stirred solution of 1-(2-pyrimidinyl)-4-piperazinyl propanol 3 g. (0.013 mol) in 50 mol. of dimethylformamide was added 3.3 g. (0.013 mol) of diphenylmethylbromide and 2.9 g. (0.034 mol) of sodium bicarbonate. The reaction mixture was refluxed overnight, dimethylformamide was evaporated under reduced pressure, and the residue was extracted with methylene chloride (400 ml.). The methylene chloride extracts were collected, washed with water and evaporated, and the remaining residue was purified by HPLC to give 1.3 g. (26% yield) of the title compound. The free base which was converted to the (1:1) fumarate salt; m.p 166°-168° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04766215uspto-grants-1988_08